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目的对注射用盐酸吉西他滨的主要杂质进行结构分析。方法采用液相色谱-四级杆飞行时间质谱联用技术对该杂质进行结构分析,色谱条件:采用ZORBAX Eclipse XDB-C18(4.6 mm×250 mm,5μm)色谱柱,以甲醇-10 mmol·L-1醋酸铵溶液(用醋酸调节pH至5.7))(1∶9)为流动相,流速1.0 mL·min-1;质谱条件:正离子检测模式,毛细管电压:4.0 kV,锥孔电压:65 V,喷雾气压:310 kPa,干燥气(氮气)流量:11 L·min-1,干燥气温度:350℃,碎裂电压150 V;结吉西他滨与该杂质的多级质谱裂解规律,研究质谱碎片裂解途径,鉴定该杂质的结构。。结果该未知杂质为2'-脱氧-2',2'-二氟尿苷。结论本实验为药物的杂质控制和工艺优化提供参数,进而提高用药安全性。
Objective To analyze the major impurities of gemcitabine hydrochloride for injection. Methods The structure of this impurity was analyzed by liquid chromatography-quadrupole time-of-flight mass spectrometry. The chromatographic conditions were as follows: using a ZORBAX Eclipse XDB-C18 column (4.6 mm × 250 mm, 5 μm) -1 ammonium acetate solution (adjusted to pH 5.7 with acetic acid)) (1: 9) as the mobile phase with a flow rate of 1.0 mL · min -1. MS conditions: positive ion detection mode, capillary voltage: 4.0 kV, V, spray pressure: 310 kPa, flow rate of dry gas (nitrogen): 11 L · min-1, temperature of drying gas: 350 ℃, fragmentation voltage of 150 V; multi-stage mass spectrometric cleavage of gemcitabine and the impurity Cleavage pathway to identify the structure of the impurity. . As a result, this unknown impurity is 2'-deoxy-2 ', 2'-difluorouridine. Conclusion This experiment provides parameters for drug impurity control and process optimization, thereby improving the safety of medication.